JPH0587797A - Analyzing method of distribution of molecular weight of high-molecular weight polyacrylamide - Google Patents
Analyzing method of distribution of molecular weight of high-molecular weight polyacrylamideInfo
- Publication number
- JPH0587797A JPH0587797A JP25070691A JP25070691A JPH0587797A JP H0587797 A JPH0587797 A JP H0587797A JP 25070691 A JP25070691 A JP 25070691A JP 25070691 A JP25070691 A JP 25070691A JP H0587797 A JPH0587797 A JP H0587797A
- Authority
- JP
- Japan
- Prior art keywords
- molecular weight
- gpc
- phosphoric acid
- acid buffer
- weight polyacrylamide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、重量平均分子量が1千
万を越える高分子量ポリアクリルアミドの分析法に関す
る。さらに詳しくは、ゲルパーミェーションクロマトグ
ラフ(以下、GPCという)を用いた高分子量ポリアク
リルアミドの品質管理、性能評価に関する。TECHNICAL FIELD The present invention relates to a method for analyzing high molecular weight polyacrylamide having a weight average molecular weight of more than 10 million. More specifically, it relates to quality control and performance evaluation of high molecular weight polyacrylamide using gel permeation chromatograph (hereinafter referred to as GPC).
【0002】[0002]
【従来技術】ポリアクリルアミドで特に重量平均分子量
が1千万を越える高分子量のものは、耐磨耗性、耐熱
性、耐薬品性に優れ、高機能材料として各種の用途が開
発されている。2. Description of the Related Art Polyacrylamides, especially those having a high molecular weight exceeding 10 million in weight average molecular weight, are excellent in abrasion resistance, heat resistance and chemical resistance, and have been developed for various uses as high-performance materials.
【0003】したがって、かかる材料に使用するために
も、その品質管理、性能評価等が必要で、高分子量ポリ
アクリルアミドの分子量分布の分析をすることが望まれ
ている。そのため、従来は、かかるポリアクリルアミド
を、100mM程度の硝酸ナトリウム、塩化カリウムに
溶解して、該溶液を硝酸ナトリウム、塩化カリウムなど
を移動相としてGPCで分析することを行っていた。Therefore, quality control, performance evaluation, etc. are required for use in such materials, and it is desired to analyze the molecular weight distribution of high molecular weight polyacrylamide. Therefore, conventionally, such polyacrylamide was dissolved in about 100 mM of sodium nitrate and potassium chloride, and the solution was analyzed by GPC using sodium nitrate, potassium chloride and the like as a mobile phase.
【0004】[0004]
【発明が解決しようとする課題】しかしながら、従来法
においては、高分子量ポリアクリルアミドの硝酸ナトリ
ウム、塩化カリウムへの溶解性が乏しく、クロマトグラ
ムが再現しないという難点があった。そのため、正確に
高分子量ポリアクリルアミドの品質管理、性能評価等が
できず、製品になった時点で材料に欠陥があることが初
めてわかることが多々あった。However, in the conventional method, there is a problem that the chromatogram cannot be reproduced because the high molecular weight polyacrylamide has poor solubility in sodium nitrate and potassium chloride. Therefore, quality control and performance evaluation of high molecular weight polyacrylamide could not be performed accurately, and it was often the first time that it was found that the material had defects when it was made into a product.
【0005】そこで、本発明は、高分子量ポリアクリル
アミドを溶解させる新たな溶媒を見出だすことにより、
前記課題を一挙解決することを目的とする。Therefore, the present invention was found to find a new solvent for dissolving high molecular weight polyacrylamide,
It is an object of the present invention to solve the above problems all at once.
【0006】[0006]
【課題を解決するための手段】本件発明者は、上記課題
を解決するため、鋭意検討した結果、高分子量ポリアク
リルアミドがりん酸緩衝液に非常に良く溶解することを
見出し、本発明をなすに至った。Means for Solving the Problems The inventors of the present invention have made extensive studies to solve the above problems, and as a result, have found that high molecular weight polyacrylamide dissolves very well in a phosphate buffer, and therefore, the present invention is made. I arrived.
【0007】すなわち、本発明は、高分子量ポリアクリ
ルアミドをりん酸緩衝液で溶解した後、該溶液をりん酸
緩衝液を移動相とするゲルパーミェエーションクロマト
グラフに付して分析することを特徴とする。That is, the present invention is characterized in that a high molecular weight polyacrylamide is dissolved in a phosphate buffer solution and then the solution is subjected to gel permeation chromatography using a phosphate buffer solution as a mobile phase for analysis. And
【0008】ここで、りん酸緩衝液の濃度は、クロマト
グラムが再現できる程度高分子量ポリアクリルアミドを
溶解させる濃度のものでなければならず、具体的には、
200mM〜400mMの範囲のものが好ましい。この
範囲のより少なければ、溶解性が落ち、この範囲を越え
ると溶解性は変わらないからである。りん酸緩衝液のp
Hは、特に制約はないが、カラム劣化防止の観点から弱
酸性域から中性域のものが好ましい。りん酸緩衝液自体
は、市販のものをそのまま使用しても、精製して用いて
もどちらでも良い。Here, the concentration of the phosphate buffer must be such that high molecular weight polyacrylamide can be dissolved to such an extent that the chromatogram can be reproduced.
The range of 200 mM-400 mM is preferable. If the content is less than this range, the solubility will decrease, and if it exceeds this range, the solubility will not change. P of phosphate buffer
H is not particularly limited, but is preferably in the weakly acidic range to the neutral range from the viewpoint of preventing column deterioration. The phosphate buffer solution itself may be a commercially available one or may be purified and used.
【0009】りん酸緩衝液に高分子量ポリアクリルアミ
ドを溶解させるには、例えば、高分子量ポリアクリルア
ミドをビーカーに入れ、そこにりん酸緩衝液の適当量を
加えるだけでよいが、その手法は問わない。溶解に必要
なりん酸緩衝液の量は、試料量に左右されるのは勿論で
あるが、クロマトグラムが再現できる程度の溶解の割合
は、0.1重量%程度である。In order to dissolve the high molecular weight polyacrylamide in the phosphate buffer solution, for example, the high molecular weight polyacrylamide may be placed in a beaker and an appropriate amount of the phosphate buffer solution may be added thereto, but the method is not limited. .. The amount of the phosphate buffer required for the dissolution depends on the amount of the sample, but the dissolution rate at which the chromatogram can be reproduced is about 0.1% by weight.
【0010】りん酸緩衝液に高分子量ポリアクリルアミ
ドを加えると、高分子量ポリアクリルアミドが溶解して
き、それをGPCに付す。GPCに付すには、公知の試
料導入装置を使用でき、これにより、所定量の溶液をG
PCに注入できる。When high molecular weight polyacrylamide is added to the phosphate buffer, the high molecular weight polyacrylamide dissolves and is subjected to GPC. A well-known sample introduction device can be used to attach to GPC.
Can be injected into a PC.
【0011】GPCに注入された溶液は、りん酸緩衝液
を移動相として分離カラムに付される。ここで、GPC
の移動相と溶解用の溶液とは同一であることが装置の操
作上好ましい。The solution injected into GPC is applied to a separation column using a phosphate buffer as a mobile phase. Where GPC
It is preferable for the operation of the apparatus that the mobile phase and the solution for dissolution are the same.
【0012】GPCで用いる分離カラムとしては、汎用
の高分子ゲルを充填したものが使用可能であり、例え
ば、ビニルアルコールコポリマーの充填カラムが好適な
例として挙げられる。As the separation column used in GPC, a column packed with a general-purpose polymer gel can be used. For example, a packed column of vinyl alcohol copolymer can be mentioned as a suitable example.
【0013】また、GPCの検出手段としては、例え
ば、示差屈折率検出器を用いるのが好ましい。As the GPC detecting means, for example, a differential refractive index detector is preferably used.
【0014】[0014]
【作用】本発明によれば、高分子量ポリアクリルアミド
の溶解性が良くなるので、GPCでのクロマトグラムの
再現性が良くなる。According to the present invention, the solubility of high molecular weight polyacrylamide is improved, and thus the reproducibility of the chromatogram by GPC is improved.
【0015】[0015]
【実施例】本発明の方法を実施する装置構成を図面に基
づいて説明する。図1は、本発明の方法を実施する装置
の一例で、1は移動相貯流槽、2は送液ポンプ、3はマ
ニュアルインジェクタ、4はカラム、5はカラムオーブ
ン、6は示差屈折率検出器、7はデータ処理装置であ
る。DESCRIPTION OF THE PREFERRED EMBODIMENTS An apparatus configuration for carrying out the method of the present invention will be described with reference to the drawings. FIG. 1 shows an example of an apparatus for carrying out the method of the present invention, 1 is a mobile phase reservoir, 2 is a liquid feed pump, 3 is a manual injector, 4 is a column, 5 is a column oven, and 6 is a differential refractive index detection. A container 7 is a data processing device.
【0016】分析に際しては、移動相貯流槽1からポン
プ2によりあらかじめ移動相を流し、定常状態を作る。
次に、マニュアルインジェクタ3から試料を注入する。
注入された試料は移動相によりカラムオーブン5中のカ
ラム4に送られ、検出器6により検出される。このデー
タをデータ処理装置7で処理し、定量計算を行う。In the analysis, the mobile phase is preliminarily flowed from the mobile phase storage tank 1 by the pump 2 to create a steady state.
Next, the sample is injected from the manual injector 3.
The injected sample is sent to the column 4 in the column oven 5 by the mobile phase and detected by the detector 6. This data is processed by the data processing device 7, and quantitative calculation is performed.
【0017】以上の装置を用いて、次の分析条件で分析
を行った。 (1)試料の調整 高分子量ポリアクリルアミドを200mMりん酸緩衝液
で溶解後、その200μlをGPCに注入する。Using the above apparatus, analysis was conducted under the following analysis conditions. (1) Preparation of sample After dissolving high molecular weight polyacrylamide in 200 mM phosphate buffer, 200 μl of the solution is injected into GPC.
【0018】(2)分析条件 カラム:Asahipak GS−710H((株)島
津製作所製) (7.6mmI.D.×250mml) 移動相:200mMりん酸緩衝液 流 量:1.0ml/min 温 度:40℃ 検出器:RID−6A(示差屈折率検出器 (株)島津
製作所製) 感 度:64×10-6 RIUFS ポラリティ:+ (3)分析結果 上記分析条件で分析した結果を図2に示す。この図より
本発明によれば、高分子量ポリアクリルアミドがGPC
で感度良く分析できることがわかる。図2中の縦軸は信
号強度、横軸は保持時間を表す。(2) Analytical conditions Column: Asahipak GS-710H (manufactured by Shimadzu Corporation) (7.6 mm ID × 250 mml) Mobile phase: 200 mM phosphate buffer Flow rate: 1.0 ml / min Temperature : 40 ° C. Detector: RID-6A (Differential Refractive Index Detector manufactured by Shimadzu Corporation) Sensitivity: 64 × 10 −6 RIUFS Polarity: + (3) Analysis results The results of analysis under the above analysis conditions are shown in FIG. Show. From this figure, according to the present invention, high molecular weight polyacrylamide
You can see that you can analyze with high sensitivity. The vertical axis in FIG. 2 represents the signal intensity and the horizontal axis represents the holding time.
【0019】[0019]
【発明の効果】本発明によれば、高分子量ポリアクリル
アミドの分析を効率良く、正確に行うことができる。さ
らに、得られた分子量分布により高分子量ポリアクリル
アミドの品質管理、性能評価が簡単に行えるという特別
の効果を有する。According to the present invention, high molecular weight polyacrylamide can be analyzed efficiently and accurately. Further, the obtained molecular weight distribution has a special effect that quality control and performance evaluation of high molecular weight polyacrylamide can be easily performed.
【図1】本発明の構成を実施するための装置を示す図FIG. 1 shows an apparatus for implementing the arrangement of the invention.
【図2】本発明の方法により分析した結果を示す図FIG. 2 is a diagram showing the results of analysis by the method of the present invention.
1:移動相貯流槽 4:分析カラム 6:検出器 1: Mobile phase storage tank 4: Analytical column 6: Detector
Claims (1)
衝液で溶解した後、該溶液をりん酸緩衝液を移動相とす
るゲルパーミェエーションクロマトグラフに付して分析
することを特徴とする高分子量ポリアクリルアミドの分
子量分布分析法。1. A high-molecular-weight polymer characterized by dissolving a high-molecular-weight polyacrylamide in a phosphate buffer and then subjecting the solution to gel permeation chromatography using a phosphate buffer as a mobile phase for analysis. Molecular weight distribution analysis method for polyacrylamide.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP25070691A JPH0587797A (en) | 1991-09-30 | 1991-09-30 | Analyzing method of distribution of molecular weight of high-molecular weight polyacrylamide |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP25070691A JPH0587797A (en) | 1991-09-30 | 1991-09-30 | Analyzing method of distribution of molecular weight of high-molecular weight polyacrylamide |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH0587797A true JPH0587797A (en) | 1993-04-06 |
Family
ID=17211839
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP25070691A Pending JPH0587797A (en) | 1991-09-30 | 1991-09-30 | Analyzing method of distribution of molecular weight of high-molecular weight polyacrylamide |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH0587797A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102749411A (en) * | 2012-07-11 | 2012-10-24 | 中国烟草总公司郑州烟草研究院 | Determination method for acrylamide in main stream smoke of cigarette |
CN114441661A (en) * | 2020-11-03 | 2022-05-06 | 中国石油化工股份有限公司 | Method for measuring content of polyacrylamide network structure |
-
1991
- 1991-09-30 JP JP25070691A patent/JPH0587797A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102749411A (en) * | 2012-07-11 | 2012-10-24 | 中国烟草总公司郑州烟草研究院 | Determination method for acrylamide in main stream smoke of cigarette |
CN114441661A (en) * | 2020-11-03 | 2022-05-06 | 中国石油化工股份有限公司 | Method for measuring content of polyacrylamide network structure |
CN114441661B (en) * | 2020-11-03 | 2023-09-12 | 中国石油化工股份有限公司 | Method for measuring content of polyacrylamide network structure |
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